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CARBOTHERMIC REDUCTION of MECHANICALLY ACTIVATED Nio-CARBON MIXTURE: NON-ISOTHERMAL KINETICS

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CARBOTHERMIC REDUCTION of MECHANICALLY ACTIVATED Nio-CARBON MIXTURE: NON-ISOTHERMAL KINETICS J. Min. Metall. Sect. B-Metall. 54 (3) B (2018) 313 - 322 Journal of Mining and Metallurgy, Section B: Metallurgy CARBOTHERMIC REDUCTION OF MECHANICALLY ACTIVATED NiO-CARBON MIXTURE: NON-ISOTHERMAL KINETICS S. Bakhshandeh, N. Setoudeh *, M. Ali Askari Zamani, A. Mohassel Yasouj University, Materials Engineering Department, Yasouj, Iran (Received 23 March 2018; accepted 10 December 2018) Abstract The effect of mechanical activation on the carbothermic reduction of nickel oxide was investigated. Mixtures of nickel oxide and activated carbon (99% carbon) were milled for different periods of time in a planetary ball mill. The unmilled mixture and milled samples were subjected to thermogravimetric analysis (TGA) under an argon atmosphere and their solid products of the reduction reaction were studied using XRD experiments. TGA showed that the reduction of NiO started at ~800 and ~720 in un-milled and one-hour milled samples respectively whilst after 25h of milling it decreased to about 430 . The kinetics parameters of carbothermic reduction were determined using non-isothermal method (Coats-Redfern Method) for un-milled and milled samples. The activation energy was determined to be about 222 kJ mol -1 for un-milled mixture whilst it was decreased to about 148 kJ mol -1 in 25-h milled sample. The decrease in the particle size/crystallite size of the℃ milled samp℃les resulted in a significant drop in the reaction temperature. ℃ Keywords : Ball milling; Carbothermic reduction; Nickel oxide; Non-isothermal kinetics; Thermo-gravimetric analysis (TGA). 1. Introduction solid product catalyzes the reaction rate [ 11 ]. It has been shown that mechanical activation by There have been many investigations on the milling reactants together with extended periods of carbothermic reduction of metal oxide in the literature time can intensify the reactions [ 16-19 ]. During and the mechanism of this reaction has been the mechanical activation and ball milling processes, the subject of intense research [ 1-5 ]. Recently, the use of reactant materials are intimately mixed at the solar energy for production of metals from their nanoscale. Previous works have indicated the rate of oxides with carbothermal process has been a subject carbothermic reduction reactions can be greatly of the study to optimize the carbothermal reduction of increased by pre-milling the mineral and carbon MgO using concentrated solar energy in low vacuum together compared to with powders milled separately conditions [ 6]. Several mechanisms have been and then mixed [ 16-19 ]. The effect of mechanical proposed to explain the carbothermic reduction activation and extended milling on the carbothermic between two solid reactants (such as oxide and reduction of manganese ore [ 18 ], ilmenite [ 20 ], carbon) and the formation of solid metal. The oldest hematite [ 21 ], titanium oxides [ 22 ] celestite [ 19 , 23 ], and most widespread mechanism in this regard is the and carbonitridation of zircon [24] have been studied oxide reduction through gaseous intermediate CO (g) recently. The results show that, generally, the longer and CO 2 in accordance with the following reactions the samples are milled together the greater the extent [7]: of reaction at lower temperatures is [ 24 ]. Reduction of MO+Æ+ CO M CO nickel oxide by graphite during ball milling at both ()sg ( ) () s2 (1) ambient and elevated temperatures has been studied C + (s CO2 +Æ C()sg2 CO ( ) by Yang and McCormick [ 25 ]. Their results showed (2) that milling significantly reduced the critical reaction N + (g The carbothermic reduction of nickel oxide and temperature for reduction [ 25 ]. reduction of NiO with CO (g) have been studied under There are many research works about the different conditions by many researchers [ 8-15 ]. It has carbothermic reduction of nickel oxide. However, the been reported that the reduction of NiO is attributed to kinetics of reduction reaction between NiO and the special class of solid-state reactions where the carbon has been studied under an isothermal condition a *Correspon d i n g a u t h o r : n s e t o u d e h @ y u . a c . i r a a DOI:10.2 2 9 8 / J M M B 1 8 0 3 2 3 0 2 2 B a a a [ [ [ [ [ [ a a [ [ 1 1 - - ( ( 1 1 1 1 3 1 3 1 314 S. Bakhshandeh et al. / JMM 54 (3) B (2018) 313 - 322 in the previous works [ 8, 11-14 ]. Reduction of nickel thermogravimetric analyzer (BAHR thermoanalyzer- oxide with carbon, polyethylene, and polystyrene has STA503-GmbH). Physical mixtures of raw materials been investigated under non-isothermal conditions in (NiO-Carbon active) was prepared in accordance with the temperature range 20-1000 . The authors the stoichiometric mixture given by reaction (3) in indicated that at heating rates of 5-20 K/min, both order to study the carbothermic reduction in the un- carbon and polyethylene reduce nickel oxide. milled samples, Moreover, they determined that the effective All solid products were analyzed using X-ray activation energies of NiO reductio℃n with carbon are diffraction (XRD, Philips Analytical, Co-K α about 284 kJ mol -1 (68 kcal mol -1 ) [ 15 ]. radiation, 40 kV, 40 mA, X’Pert APD) over a 2 θ range The present work was conducted in order to study of 20-100° and 2 sec count time for every 0.05° step. the effects of mechanical activation on the The microstructures of the as-milled and the heated carbothermic reduction of nickel oxide with activated samples were studied using a scanning electron carbon. The aim of this work is to investigate the microscope (TESCAN-VEGA3). The crystallite size kinetics of carbothermic reduction of nickel oxide of solid products in the as-milled samples was under non-isothermal conditions for un-milled determined using the well-known Scherrer equation. mixture and milled samples. The kinetics parameters for both un-milled and milled samples are determined 3. Results and discussion using Coats-Redfern method. Moreover, the 3.1 Characterization of mixtures fundamental characteristics of both un-milled mixture and milled samples are examined using TGA, XRD, Fig. 1 illustrates the XRD patterns of the as-milled and SEM analyses. samples for different milling times. The major peaks of NiO (JCPDS card file No. 71-1179) were clearly 2. Experimental observed in the 25h as-milled sample. Therefore, based on the XRD results in Fig. 1, reduction of nickel The characteristics of starting materials (nickel oxide by carbon active cannot occur after 25h milling. oxide and carbon active with purity of 99%) are listed Thermodynamic calculations [ 26-27 ] indicate that in Table 1. The amount of ash for carbon active was reaction (3) is endothermic and feasible at less than 1%. Stoichiometric mixtures of NiO-Carbon temperatures above of 440 . Therefore, the signs of (86.148 wt.% of NiO and 13.852 wt.% of carbon NiO in the XRD patterns of as-milled samples (Fig.1) active) were prepared based on reaction (3). clearly show that the temperature of solid mixtures in NiO+Æ C Ni + CO the milling vial can never reach 440 ()g (3) The broadening ℃of the main peak of NiO at È g Tl hermodynamic calculations indicate the value of 2 50.7° (d=2.08794Å, 200) with increasing milling ΔG0 for reaction (3) is negative at a temperature above time (Fig. 1) may be related to the reduction of mean ~440 at standard conditions [ 26,27 ]. crystallite size. It is worth noting ℃th aatf treerd 2uc5t ihoonu rosf omfe manil clirnygs.t allite size of particles and amorphization, a Table 1. The characteristics of starting materials. well-known phenomenon during high-energy ball a milling, results in not only decreased peak intensity Characteristic Nickel oxide (NiO) Carbon active but broadening of the peak width as well [ 28-29 ]. of m℃ater i a l s a Table 2 lists the mean crystallite sizes of the nickel Colou r b l a c k b l a cak oxide for different milling times. The crystallite size Structure Cubic (JCPDS-71-1179) amorphous [ of nickel phase was determined using Scherrer d(0.1) = 0.86 d(0.1) = 4.961 equation based on its main peak (i.e., 2=50.705). The Size analyses d(0. 5 ) = 6 . 1 5 3 d ( 0 . 5 ) = [ 18.806 results in Table 2 show that with increasing milling (m) d(0.9 ) = 2 4 . 8 0 5 d ( 0 . 9 ) = [ 58.392 time, the crystallite size of nickel oxide decreases and reaches about 20 nm in 25h milled sample. The st o i c h i o m e t r i c m i x t u r e s w e r e m e c h aanically milled in a closed chamber using a planetary ball mill Table 2. The values of crystallite size of nickel oxide and [ percent of iron contamination in the as-milled (Farapazhouhesh, FP2 model) for different milling samples with increasing milling times. times. The milling c o n d i t i o n s f o r a l l r u n s 1were: a rotation speed of 600 rpm, high-chromium steel balls Milling time Crystallite size Amount of Iron - (20 mm diameter), high-chromium steel milling (hr.) (nm) (in ppm) ( chamber, and the ball-to-powder weight ratio of 40:1. 1 38.76 6.61 Thermograv i m e t r i c a n a l y s i s ( T G A ) w a s c a r r i1ed 1out 5 28.91 12.41 on the NiO-carbon mixtures at the heating rate of 10 10 25.56 11.54 C/m3in up t o 1 , 2 0 0 u n d e r t h e f l o w o f 1argon 15 25.78 13.92 (99%purity, flow rate of 5 mL/min) using a 25 19.84 14.72 ℃ S.
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